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Hydrochloric Acid → Salmeterol

HRID 1936219
ノート
印刷プレビュー

反応式

HRID 1936219 の反応式
CC1(C)[O:7][CH2:6][C:5]2[CH:8]=[C:9]([CH:12]([OH:32])[CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH:10]=[CH:11][C:4]=2[O:3]1.Cl>O.CO>[OH:7][CH2:6][C:5]1[CH:8]=[C:9]([CH:12]([OH:32])[CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:10]=[CH:11][C:4]=1[OH:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 101827471-(2,2-dimethyl-4H-benzo[d][1,3]dioxin-6-yl)-2-(6-(4-phenylbutoxy)hexylamino)ethanol

生成物 1

HCID 5152Salmeterol収率 43.9%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

To a solution of 0.6 g (1.32 mmol) [2-(2,2-dimethyl-4H-benzo[1,3]dioxin-6-yl)-2-hydroxyethyl]-6-[4-phenylbutoxy)hexylamine in 20 ml of a 1:1 H2O/MeOH mixture is added 0.15 ml (1.75 mmol) 35% HCl. After allowing the reaction to stir for 48 hr at room temperature, the MeOH is evaporated off at reduced pressure. The resulting aqueous mixture is extracted with 20 ml CH2Cl2. The organic phase is washed sequentially with 20 ml of a saturated NaHCO3 solution and further 20 ml H2O, dried on anhydrous Na2SO4 and evaporated to dryness to yield 0.24 g (43.9%) 2-hydroxymethyl-4-{1-hydroxy-2-[6-(4-phenylbutoxy)hexylamino]ethyl}phenol.

後処理

  1. customthe reaction
  2. customthe MeOH is evaporated off at reduced pressure
  3. extractionThe resulting aqueous mixture is extracted with 20 ml CH2Cl2
  4. washThe organic phase is washed sequentially with 20 ml of a saturated NaHCO3 solution and further 20 ml H2O
  5. dry with materialdried on anhydrous Na2SO4
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-572e128e9e484081a5dc01f09c3e2226
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06388134B1

反応ノート

読み込み中…

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